Dataset for "Continuous flow for materials synthesis, assembly and crystallisation at Diamond: discovery and delivery of high value materials"

  • Lois Wayment (Creator)
  • Chick Wilson (Supervisor)
  • Karen Robertson (Supervisor)
  • Mark R Warren (Supervisor)
  • David R. Allan (Supervisor)
  • Chiu Tang (Supervisor)
  • Daniel Scott (Contributor)
  • Mark Levenstein (Contributor)
  • Pollyanna Payne (Contributor)
  • Ruth Lunt (Contributor)
  • Pierre-Baptiste Flandrin (Contributor)

Dataset

Description

Continuous crystallisation of the model system Carbamazepine (CBZ) in ethanol in the KRAIC-D (Kinetically Regulated Automated Input Crystalliser - Diffraction) platform on beamline I11 (high resolution powder diffraction) is presented. The effect of introducing a controlled solid interface into the crystallisation process is investigated, where CBZ form III seeds are introduced in polymorphic purity at different seeding positions (pre- and post-nucleation) throughout the length of the KRAIC-D. The video associated with Chapter 4 corresponds with a post-nucleation CBZ form III experiment where a separation of crystal habit is observed as a result of the different interaction with the flow paths in the solution slugs with the segmented flow.

The second device is the KRAIC-S (Kinetically Regulated Automated Input Crystalliser - Single Crystal) platform installed at I19 (small molecule single crystal beamline) employed to investigate the continuous crystallisation of paracetamol (PCM) in 60:40 water:isopropanol via a range of experiments including unseeded and seeded cooling crystallisations. The unseeded experiments also looked at the crystallisation at different set points along the KRAIC-S (6.7 m and 8.7 m) to investigate crystal growth and crystal rotation at different length scales. The videos associated with Chapter 5 include single crystals produced from the range of experiments investigated. Each video tracks a different single crystal in a solution slug, where through use of the slug triggering mechanism, whereby an optical trigger prompts translation of the motorised stage to artificially suspend the single crystal in the X-ray beam during data collection. These videos complement the diffraction data and can provide explanation for data collections, which do not achieve cell indexation as the single crystal is shown to move in and out of the X-ray beam in these videos.
Date made available1 Jun 2020
PublisherUniversity of Bath

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